CEB 2072 – Chemical Engineering Lab II

May 2022 Semester

Laboratory Report 2

09/06/2022

Chemical Engineering Department

Experiment 7: Gas Diffusion Coefficient

Lab Instructor: Sir Mahesh Chandra

BY GROUP 2F:

Group Members Student ID

Nur Shahirah Binti Shaifol Azman 19001142

Nur Intan Syahirah Binti Suhaifa 19001391

Muhammad Haziq Mirza Bin Saidi 19001323

Aelieya Shahira Binti Ayub 19001104

Mohamad Akil Najmi Bin Md Romzi 19001301

 EXECUTIVE SUMMARY

Gas diffusion is a mass transfer application in which the studied substance in a gas
phase goes from locations of high partial pressure to areas of low partial pressure. This
mechanism is driven by partial pressure, which changes the rate of diffusion of the studied
substance. In this paper, the diffusion of acetone is studied where the theoretical value of
diffusivity is compared with the value calculated using Stefan-Winkelmann method. The
Stefan-Winkelmann method, which is commonly used to assess the diffusivity of a volatile
liquid, takes into account the rate of evaporation of the volatile liquid, which is then followed
by the rate of descent of the liquid surface in a glass tube or diffusion cell (Coca et al., 1980).
Acetone is a volatile compound that evaporates at room temperature under normal conditions.
In this experiment, the Winkelmann method is employed to determine the diffusivity of
acetone. The tube capillary has been filled with liquid acetone, and a pressure pump functions
as the driving force in the tube. The acetone diffused as a result of this experimental setup, and
the diffusivity was determined using the Winkelmann method and compared to the theoretical
value acquired from a credible research publication. It can be observed that the value obtained
using Winkelmann method differs from the theoretical value because an error occurred during
the experimental phase, resulting in a 98.09 percent percentage error. The error, which includes
parallax error and bubble in the tube, can be prevented by taking precautionary measures such
as ensuring that the eye is perpendicular to the reading scale and that no bubble escapes from
the tube while the experiment is carried out. It can be said that Winkelmann method is a reliable
method to measure diffusivity of the volatile liquid because it considers the evaporation of the
substance while the experiment is conducted.
 TABLE OF CONTENTS

No. Content Page

1. Introduction & Objectives 1

2. Methodology/Experimental procedures 4

3. Results & Discussion 10

4. Conclusion 16

5. Reference 17

6. Appendix 19
 01 INTRODUCTION

1.1 Introduction
Mass transfer is referred to as the movement of fluid components in a direction that
reduces the concentration gradient exists between two or more components in a fluid. To
put it simply, mass transfer by diffusion is the movement of mass caused by the differences
in concentration of the species in a mixture. Mass transfer can occur in either a gas or a
liquid phase, or both phases at the same time. According to Reisfeld (2021), a concentration
gradient is a difference in the abundance of chemical species across time. Mass transfer by
diffusion is usually faster in the gas phase rather than in the liquid phase because liquid
molecules are firmly packed together, limiting the movement of the molecules. Illustration
of the mechanism of concentration gradient is shown in Figure 1 below.

Figure 1: Concentration Gradient

Diffusivity of a substance can be obtained from Fick’s law of diffusion. According
to Fick’s law of diffusion, the molar flux due to diffusion of a substance across a unit area
is directly proportional to the concentration gradient (Davis, Parbrook & Kenny, 1995).
This means that as the concentration gradient between two adjacent regions increases, the
rate of diffusion of a substance also increases. Fick’s laws of diffusion can be divided into
two categories: (i) Fick’s first law of diffusion and (ii) Fick’s second law of diffusion.
According to Libretexts (2021), the first law can only be applied to systems if the flux
coming into the system equals the flux going out, but the second law can be applied to
systems when the flux going in is not equal to the flux going out.
Stefan-Winkelmann technique is used to measure the diffusivities of vapours by
determining the rate of evaporation of a volatile liquid, followed by the rate of fall of the
liquid surface in a glass tube or diffusion cell (Coca, Bueno & Alvarez, 1980). This
experiment is designed to determine the diffusivity of acetone (volatile liquid) in air at the

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temperature of 55 °C and atmospheric pressure by using the established Winkelmann’s
method. Acetone is allowed to evaporate in a glass capillary tube with an air stream passing
through the top of the tube at a rate that maintains the partial pressure of the vapour at
around zero. A water bath is utilised to keep the temperature constant during the
experiment, ensuring that mass transfer occurs only through molecular diffusion without
the presence of eddy currents. (Chhabra, 2018). The height of the liquid acetone in the
capillary tube is measured at the start of the experiment and every 15 minutes thereafter
until the 10th reading.

The rate of mass transfer can be calculated by using the following formula:
CA CT
N′A = D ( ) ( ) … … … … . (1)
L CBm
where,
D = Diffusivity [m2 /s]
CA = Saturation concentration at interface [kmol/m3]
L = Effective distance of mass transfer [m]
CT = Total molar concentration [kmol/m3]
CBm = Logarithmatic mean value of CB [kmol/m3]

By taking into account the evaporation of the liquid:

ρL dL
N′A = ( ) ( ) … … … … . (2)
M dt

where,
ρL = Density of liquid [kg/m3]
M = Molecular weight [kg/kmol]

Combining equation (1) and (2) to obtain:

ρL dL CA CT
( ) = D( )( ) … … … … . (3)
M dt L CBm

Through integration and substitution of L = Lo at t = 0, we get:

2MD CA CT
L2 − L2 0 = ( )( ) t … … … … . (4)
ρL CBm

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 Equation (4) is rearranged since L = Lo values will not be accurately measured, but (L - Lo)
values are available, thus we obtain:
2MD CA CT
(L − L0 )(L − L0 + 2L0 ) = ( )( )t
ρL CBm

or,
t ρL CBm ρL CBm
=( )( ) (L − L0 ) + ( ) L … … … … . (5)
(L − L0 ) 2MD CA CT MDCA CT 0

Slope, s can be obtained by plotting a graph of t vs (L - Lo).

ρL CBm
s=( )( ) … … … … . (6)
2MD CA CT

The diffusivity, D can be calculated by rearranging equation (6):

ρL CBm
D=( )
2MCA CT s

1.2 Objectives
The objectives of conducting this experiment are:
1. To determine the gas diffusion coefficient of acetone using the established
Winkelmann’s method.
2. To determine the diffusivity of the vapor of a volatile liquid which is acetone.

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 02 METHODOLOGY

2.1 Material and Apparatus

Figure 2.1: Material and Apparatus

Table 2.1.1: Apparatus

Item Apparatus

1) Chemical Resistant Bench

2) Electrical Control Panel

1) Main Power
2) Temperature Controller
3) Air Pump ON/OFF Switch
4) Heater ON/OFF Switch

3) Digital Analytical Balance

1) Capillary Tube Holder
2) Weighing pan
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 4) Constant Temperature Bath
1) RTD Temperature Sensor
2) Cartridge Heater
3) Level Switch

5) Glass Capillary Tube

6) Air Flow Control Valve

Table 2.1.2: Material

Item Material

1) Clean Water

2) Pure Acetone

2.2 Safety Precautious

General Safety Procedure

1) Before attempting to operate the equipment, the manual should be read and understood
properly.
2) Proper attire should be worn during laboratory session. It is highly recommended that
eye protection and gloves are used.
3) When handling hazardous material, students should be cautious and careful by always
referring to the material safety data sheet and avoiding inhalation of any hazardous
material.
4) Any spillage should be avoided onto electrical components to prevent electrical shock.
5) Experiment should be conducted in a properly ventilated room.

General Maintenance Procedure

1) The equipment should not be operated if any of the components is found to be faulty.
The manufacturer/supplier should be consulted for assistance, if needed.
2) The equipment should be disconnected from electrical supply when not in use.

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 3) The water from the water bath should be drained if the equipment is not to be used for
a long period.
4) By referring to the manufacturer’s manual equipment should be cleaned thoroughly
after use.

2.3 Experimental Procedure

2.3.1 Start-up Procedure

1) The water bath was filled with clean water to approximately 15 mm from the top.
2) The mains cable was plugged to the electrical supply and the voltage of the supply was
set correctly to suit the equipment.

Figure 2.3.1: Electrical supply plugged

3) The main power was switched on the control panel.

4) The set-point value on the temperature controller was adjusted to 50°C and not
exceeding 70°C.

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 Figure 2.3.2: Set point Value

5) The heater was switched on and as the water temperature heats up to 50°C observation
was made until it remained constant.
6) The air pump was switched on and the needle valve was adjusted so that a steady low
velocity of air stream was detected at the end of flexible tubing.
7) The equipment was ready for further experimental procedure.

2.3.2 Priming Procedure for the Capillary Tube

1) A weak solution of detergent was prepared.

2) Using a Hirschmann pipette, the tube solution was filled. The outside of the tube was
tapped when the solution is trapped and does not flow down.
3) The tube was turned upside-down and was shook. Then, the tube was emptied.
4) The steps 2 to 3 were repeated with acetone.
5) The tube was ready for further experimental procedure.

2.3.3 Experiment Procedure : Determination of the gas diffusion coefficient of acetone

using the established Winkelmann’s method

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1) The start-up procedure was performed.
2) The air pump was switched off.
3) The capillary tube was partially filled with acetone to a depth of about 30 mm (3cm).
The two capillary tube ends was closed with the cap provided.

Figure 2.3.3: Acetone was measured

4) The capillary tube was carefully inserted through the fitting on top of the water bath
cover while making sure that the fitting was not over-tightened.
5) The initial height or level of acetone filled (L0) at time, t=0 was recorded.
6) Both caps were removed and the flexible tubing was connected from the air pump line
to one end of the capillary tube. The air pump was switched on.
7) The height or level of acetone filled (L) for every 15 minutes interval was recorded
until up to 10 readings.
8) The table was filled with the data obtained and calculated.
9) Graph t/(L0 – L) against (L0 – L) was plotted and the gas diffusivity, D was determined
from the obtained slope, s.
10) The experiment value was compared with the theoretical value that could be predicted
from empirical equations (e.g. modified Maxwell’s equation by Gililand).

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2.3.4 Shut –down Procedure

1) The heater and air pump were switched off.

2) The set-point value of the temperature controller was adjusted to approximately 5
degree below the room temperature.
3) The water was cooled down until it is safe to touch. The drain valve and the water tank
were opened.
4) The flexible tubing was detached and the capillary tube was cleaned for next use.
5) The main power was switched off. The main cable was unplugged.

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 03 RESULTS & DISCUSSION

3.1 Results
Table 3.1.1: Change of liquid level in capillary tube data

Time,t (ks) Lo (mm) L (mm) Liquid Fall, t/ (Lo – L)

(Lo – L) (mm) (ks/mm)
0 30 0 0
0.9 30 0 0
1.8 30 0 0
2.7 29 1 2.7
3.6 26 4 0.9
4.5 30 26 4 1.125
5.4 24 6 0.9
6.3 23 7 0.9
7.2 22 8 0.9
8.1 20 10 0.81
9.0 18 12 0.75

t/(Lo-L) vs (Lo-L)
3

2.5

2
t/ (Lo-L)

1.5 y = 0.024x + 0.7033

R² = 0.0183
1

0.5

0
0 2 4 6 8 10 12 14
Lo-L)

Figure 3.1.1: Graph t/(Lo-L) vs (Lo-L)

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Calculations

Slope of the graph, s = 0.024 ks/mm2

0.024 𝑘𝑠 1000𝑠 (10002 𝑚𝑚2 )

× ×
𝑚𝑚2 1 𝑘𝑠 1𝑚

𝑠 = 2.4 × 107 𝑠/𝑚2

Molecular weight, M(kg/kmol)

Molecular weight of acetone = 58.08 g/mol = 58.08 kg/kmol

Total molar concentration, CT (kmol/m3)

1 (𝑇𝑎𝑏𝑠 )
𝐶𝑇 = ( )
22.4 𝑘𝑚𝑜𝑙 𝑇

1 273
𝐶𝑇 = ( )
22.4 𝑘𝑚𝑜𝑙 273 + 55

𝑘𝑚𝑜𝑙
𝐶𝑇 = 0.0372
𝑚3

Vapour pressure of acetone, Psat

Vapour pressure was obtained by referring table for Antoine equation:

𝐵
𝐿𝑛𝑃 𝑠𝑎𝑡 = 𝐴 −
𝑇+𝐶

𝐵
𝑃 𝑠𝑎𝑡 = 𝑒𝑥𝑝 (𝐴 − )
𝑇+𝐶

2756.22
𝑃 𝑠𝑎𝑡 = 𝑒𝑥𝑝 (14.3145 − )
55 + 228.060

𝑃 𝑠𝑎𝑡 = 97.25

Logarithmic mean molecular concentration of vapour, CBm (kmol/m3)

𝐶𝐵1 = 𝐶𝑇

𝑘𝑚𝑜𝑙
𝐶𝐵1 = 0.372
𝑚3

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 𝑃𝑎 − 𝑃𝑣
𝐶𝐵2 = ( )𝐶𝑇
𝑃𝑎

101.3 − 97.25
𝐶𝐵2 = ( ) 0.0372
101.3

𝐶𝐵2 = 0.0015 𝑘𝑚𝑜𝑙/𝑚3

𝐶𝐵1 − 𝐶𝐵2
𝐶𝐵𝑚 = ( )
𝐶
𝑙𝑛 𝐶𝐵1
𝐵2

0.0372 − 0.0015
𝐶𝐵𝑚 = ( )
0.0372
𝑙𝑛
0.0015

𝐶𝐵𝑚 = 0.011 𝑘𝑚𝑜𝑙/𝑚3

Saturation concentration at interface, CA

𝑃𝑣
𝐶𝐵2 = ( )𝐶
𝑃𝑎 𝑇

97.25
𝐶𝐴 = ( ) 0.0372
101.3

𝑘𝑚𝑜𝑙
𝐶𝐴 = 0.036
𝑚3

Diffusivity, D (m2/s)

𝜌𝐿 = 790 𝑘𝑔/𝑚3

𝜌𝐿 𝐶𝐵𝑚
𝐷=
𝑠(2𝑀𝐶𝐴 𝐶𝑇 )

𝑘𝑚𝑜𝑙
(790 𝑘𝑔/𝑚3 )(0.011 )
𝐷= 𝑚3
𝑠 𝑘𝑔 𝑘𝑚𝑜𝑙 𝑘𝑚𝑜𝑙
(2.4 × 107 2 )(2)(58.08 )(0.036 3 )(0.372 )
𝑚 𝑘𝑚𝑜𝑙 𝑚 𝑚3

𝑚2
𝐷𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 = 2.328 × 10−7
𝑠

From the (Green & Perry, 2003), the theoretical diffusion coefficient of acetone

𝐷𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 = 1.22 × 10−5 𝑚2 /𝑠

Percentage error,

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 𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
%𝑒𝑟𝑟𝑜𝑟 = | | × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙

𝑚2
2.328 × 10−7 𝑠 − 1.22 × 10−5 𝑚2 /𝑠
%𝑒𝑟𝑟𝑜𝑟 = | | × 100%
1.22 × 10−5 𝑚2 /𝑠

% 𝑒𝑟𝑟𝑜𝑟 = 98.09 %

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3.2 Discussion

In this experiment, the gas coefficient diffusivity of acetone gas using Winkelmann’s

mass transfer theory and study concentration gradient were investigated. The objective of this

experiment is to determine value of gas diffusion coefficient using Winkelmann’s method. The

diffusion coefficient is physical constant affected by temperature and molecular size of

diffusing substance (Monstinsky, n.d.). Diffusion coefficient can also be defined as ratio of

flux density to negative concentration gradient in diffusion direction. By using gaseous

diffusivity apparatus, acetone is filled in the capillary tube until it reached 30mm and was then

connected to the air pump using flexible tubing. The height of acetone in the capillary tube

were recorded every 15 minutes interval until 10 readings are achieved. By observing the

decrease in liquid level of acetone in capillary tube, evaporation rate of acetone and diffusion

coefficient of acetone can be determined.

Using the data obtained, the ratio of the time to the different in height of acetone is

calculated and a graph is plotted and shown in Figure 3.1.1. From the result obtained, it is

observed that height of acetone for every 15 minutes of interval decrease gradually until the

final reading. Acetone evaporates, turn into vapor and diffuse through the air which have low

concentration of acetone. The slope obtained in Figure 3.1.1 is used to calculate value of

diffusivity of the acetone. From the result, the slope of the graph is 0.024 and value of

diffusivity of acetone obtained is 2.328 x 10-7 m2/s.

Thus, the aim of this experiment to achieve value of acetone diffusivity in air at

atmospheric pressure and 55 °C has been achieved. Gas diffusion is relatively rapid compared

to liquid and solid since gas molecules exhibit higher kinetic energy and their particles are

further apart from one another. Acetone diffuses through non-diffusing air, passed over the top

of tube containing acetone and the air is allowed into the tube, but does not diffuse into acetone

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(Ikrimah, 2014). The higher the difference in concentration, the quicker the rate of diffusion

(Gupta, 2020). This is due to more random collision occur on the side with higher concentration

(Rekha, n.d). The concentration gradient tends to move the component to equalize

concentration and destroy the gradient (Durga, 2014). When the gradient is maintained by

supplying the component to the high concentration end and remove it at low concentration end,

there is steady state flux which is the characteristics of many mass transfer operations (Durga,

2014).

In this experiment, value recorded for diffusion coefficient of acetone is 2.328 x 10-7

m2/s while the theoretical value is 1.22 x 10-5 m2/s. This contributes to 98.09 % of percentage

error in this experiment and this may be due to the eye level is not perpendicular to the scale

reading, causing parallax error. Besides, other cause including air bubble escaped into the tube

which affect the accuracy of data collected.

Some of precaution measures should be taken into consideration when conducting the

experiment to reduce any errors which may slightly affect the accuracy of the data. Firstly,

capillary tube containing acetone should not be taken out to maintain the temperature of

acetone which might affect the overall result. Next, while taking the reading, the eye level

should be perpendicular to the scale reading to avoid parallax error. When filling up the acetone

into the capillary tube, no air bubble should be allowed to be escaped in the tube. This can help

minimise the error and the result with more accurate data can be achieved at the end of

experiment. Appropriate attire should always be a top priority in the pilot plant laboratory.

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 04 CONCLUSION

In this experiment, the knowledge of mass transfer from Separation Process I was
covered where there are concentration gradient exists within the system of interest. The
objective of this experiment is to calculate the gas diffusion coefficient of acetone using the
well-known Winkelmann's method. The gas diffusion coefficient was calculated when the
temperature remained constant during the experiment, which was 55°C. The acetone level in
the capillary tube was measured every 15 minutes until 10 readings were acquired, and the
values were thoroughly discussed in the discussion. Based on the result, the gas diffusion
coefficient calculated using the Winkelmann’s method was significantly deviated from the
theoretical value where the percentage error was 98.09 %. This percentage error could be
caused by parallax error and an air bubble in the tube. To avoid this error, take precautionary
measures such as keeping your eye level perpendicular to the scale reading when taking any
data. Furthermore, before filling the capillary tube with acetone, make sure no air bubbles
escape.

To summarise, Winkelmann's approach is a reliable method for determining vapour

diffusivity since it takes into account the rate of evaporation of a volatile liquid, which can be
followed by the rate of fall of the liquid surface in a glass tube or diffusion cell. This experiment
requires some modification to obtain more precise and reliable results.

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 REFERENCES
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Coca, J., Bueno, J. L., & Alvarez, R. (1980). Gaseous Diffusion Coefficients by the Stefan-
Winkelmann Method Using a Polymer-Solvent Mixture as Evaporation Source.
Industrial & Engineering Chemistry Fundamentals, 19(2), 219–221.
https://doi.org/10.1021/i160074a016
Davis, P., Parbrook, G., & Kenny, G. (1995). Diffusion and Osmosis. Basic Physics and
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Durga, P.M., (2014) Department of Chemical Engineering National Institute of ... - core.
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Gupta, R. (2020, February 16). Four things that affect rate of diffusion. Sciencing., from
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Huey, J. (2017, March 30). Vapour diffusion coefficient of acetone in air KEK 150085 sin jia
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Libretexts. (2021, June 14). 9: Diffusion. Chemistry LibreTexts.

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https://www.thermopedia.com/content/696/

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Reisfeld, B. (2021). Mass Transfer — Introduction to Chemical and Biological Engineering.
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https://www.engr.colostate.edu/CBE101/topics/mass_transfer.html

Rekha. (n.d.). Factors affecting the rate of diffusion (8.1.2): Edexcel GCSE Biology Revision
Notes 2018. Save My Exams., from
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APPENDIX

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